Facile Synthesis and Characterization of Nanoporous NiO

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Materials Sciences and Applications, 2012, 3, 697-703http://dx.doi.org/10.4236/msa.2012.310102Published Online October 2012 (http://www.SciRP.org/journal/msa)

Facile Synthesis and Characterization of Nanoporous NiO

with Folic Acid as Photodegredation Catalyst for Congo

Red

Faezeh Farzaneh*, Sara Haghshenas

Department of Chemistry, University of Alzahra, Tehran, Iran.Email: *[email protected]

Received July 13th, 2012; revised August 15th, 2012; accepted September 12th, 2012

ABSTRACT

In this study nanoporous NiO was prepared using Ni(CH3COO)24H2O, folic acid and water as starting material, tem-

plate and solvent respectively, by sol gel method followed by calcination at 400C. The solid product was characterizedby X-ray diffraction (XRD), nitrogen adsorption-desorption, scanning electron microscopy (SEM), transmission elec-tron microscopy (TEM) Fourier transform infrared (FT-IR) and photoluminescence (PL) techniques. The particle size ofthe nanoparticles estimated by XRD was in good agreement with the particle size obtained by TEM analysis (4 - 5 nm).It was also found that the prepared nanoporous NiO show very good activity for photodegredation of dye organic pol-lutants such as Congo red (91%) during 1.5 hours.

Keywords:Nanoporous NiO; Photodegredation; Congo Red; Folic Acid

1. Introduction

NiO as an important transition metal oxide has received

extensive attention because of its specific structure andpotential applications in various fields, such as catalyst[1-3], battery cathodes [4], gas sensor materials [5], solarcells [6], electrochemical supercapacitors [7], electro-chromic films [8], and fuel cell electrodes [9,10]. So far,many different methods have been attempted to synthe-size nanosized NiO particles, such as thermal decompo-sition [11,12], micro emulsion [13], precipitation [14,15],electrochemical deposition [16], flame spray pyrolysisreactor [17] sol-gel technique [18,19] and surfactant me-diated method [20]. In fact nano-sized materials haveattracted much attention because of their unusual proper-ties based on size quantization effect and large surface

area [21-25].The heterogeneous photocatalysis by semiconductor

particles is newly emerging process for removal of globalenvironmental pollutants [26,27]. Various kinds of syn-thetic dyestuffs appear in the effluents of waste water insome industries such as dyestuff, textiles, leather, paper,plastics, etc. [28]. The colored effluents of waste fromthese industries can be mixed in surface water andground water systems, and then they may bring a chiefthreat to human health due to either toxic or mutagenicand carcinogenic for most of dyes [29]. Therefore, it is

necessary to remove the dye pollutions. Congo red is anexample of anionic diazo dyes and Congo red containingeffluents are generated from textiles, printing and dyeing,

paper, rubber plastics industries, etc. Due to its structuralstability, it is difficult to biodegrade. Physico-chemical orchemical treatment of such wastewaters is, however,possible [30-35].

The purpose of this study is to report the synthesis ofnanoporous NiO by sol gel process in the presence offolic acid and then was evaluated for the ability to re-move Congo red dye from aqueous solutions. The com-bined effect of adsorption-photodegredation was alsoinvestigated.

2. Experimental

2.1. Instrumentation

X-ray diffraction patterns were obtained on a PW1800diffractometer with CuK radiation (K= 0.15405 nm)and Ni-filtered. The nanostructures of the samples wereanalyzed by scanning electron microscopy (SEM; S-4160Hitachi) and transmission electron microscopy (TEM;Philips EM 208s) at an accelerating voltage of 100 kV.The photoluminescence (PL) spectrum was recorded atroom temperature using a Xe lamp with an excitationwavelength of 280 nm by a Cary Eclips-fluorescencespectrophotometer. The degradation process was ana-*Corresponding author.

Copyright 2012 SciRes.

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Facile Synthesis and Characterization of Nanoporous NiO with Folic Acid asPhotodegredation Catalyst for Congo Red

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lyzed by monitoring dye absorption intensity at themaximum absorption wavelength using a UV/vis (PerkinElmer, Lambda 35). Fourier transform infrared (FT-IR)spectra were recorded on TENSOR27 spectrophotometer

in KBr pellets. Thermal studies were performed usingMettler-Toledo TGA/SDTA-851, thermogravimetric ana-lyzer in air at a heating rate of 10C/min. Atomic ab-sorption spectrometric measurements were done using aGVC atomic absorption spectrometer.

2.2. Preparation of NiO Nanoparticles

All chemical materials were purchased from MerckChemical Company and used without further purification.In a typical synthesis, 1 mmol of Folic acid and 2 mmolof NaOH pellets were dissolved in 5 mL of water to givea homogenous solution. Then this solution was added

drop wise into 5 mL of aqueous solution containing 1mmol Ni(CH3COO)2, 4H2O under magnetic stirring for 2h. The resultant solution was refluxed for 12 h. The solidproduct was filtered, washed with distilled water to re-move the impurities, and then dried in a vacuum oven at60C for 12 h. Finally, the obtained precursor was cal-cined at 400C for 3 h. Deionized water was used formaking all solutions. The calcined solid product at 400Ccontains: Ni: 60.55%.

2.3. Photo Catalytic Activity Determination

Photocatalytic activity of the prepared NiO as photo-catalyst was evaluated by the degradation of Congo red(Scheme 1). 0.05 g of the as-prepared nano NiO waspoured into 100 mL aqueous solution of 3 ppm Congored, in a glass reaction cell. A 30 W UV-C lamp wasused as light source. The distance between the UV lampand the glass reaction cell was fixed at 8 cm. Air wasbubbled into the solution throughout the entire experi-ment to provide a constant source of dissolved oxygen.The dye solution was continuously stirred with a mag-netic stirrer. Prior to irradiation, the set up was kept inthe dark for approximately 15 minutes in order to reachan adsorption/desorption equilibrium among the photo

catalyst particles, Congo red and atmospheric oxygen.During irradiation, the degradated dye was sampled inregular intervals. The photocatalytic degradation wasmonitored by measuring the absorbance of the soltionsamples with UV-vis spectrophotometer.

NH2

SO3Na

N N N NNH2

SO3Na

Scheme 1. Structure of Congo red.

3. Results and Discussion

3.1. Characterization of Prepared NanoporousNiO

XRD analysis of the as synthesized nickel folate com-pound with folic acid and Ni(acac)2 designated as Niprecursor, followed by heating at 100C, 200C, 300C,400C for 3 h. are shown in Figures 1(a)-(e), respec-tively. Based on the obtained results at room temperatureup to 200C amorphous phases were formed, while metaloxide crystallization occurred after heat treatment at200C. By increasing temperature up to 300C and fi-nally 400C the NiO as a crystalline phase is observed.The diffracttion angle and intensity of the characteristicpeaks of the samples at 300C and 400C (Figures 1(d)and (e)) are well consistent with those of the standard

JCPDS card no (04-0835). The main diffraction peakswere observed at 2, 37.13, 43.53, 63.11, 75.80 and79.22. All diffracttion peaks can be indexed to the pureNiO crystalline phase (space group: Fm3m), no impurepeaks are observed in the XRD pattern. The average par-ticle size was about 4.8 - 5 nm determined from XRDpattern parameters of the NiO powder according to thesherrer Equation (1) [15].

0.9 cosD (1)

where (FWHM; full-width at half-maximum or half-width) is in radians and is the position of the maximumof diffraction peak (200) and is the X-ray wavelength

(1.5406 for CuK).

Figure 1. XRD patterns of (a) As prepared Ni precursor; (b)

After heat treatment at 100C; (c) 200C; (d); 300C; (e)

and 400C.


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The FT-IR spectra of folic acid, as prepared sampleafter heated at 100C, 200C and calcined at 400C areshown inFigures 2(a)-(d)respectively. The broad peakat ca. 3450 - 3400 cm1in all four spectra are representa-

tive of OH stretching vibrations of template and adsorbedwater. The vibration bands at 2946 and 2869 cm1 are dueto the CH2groups of folic acid. The FTIR of folic acid(Figure 2(a)) shows vibration at the regions 1694, 1449,1333 - 1352 and 600 cm1 due to the (C=O), as(COO-),s(COO-) and C-OH of folic acid and C-O bending vibra-tion respecttively [36]. By increasing temperature to 100,200C (Figures 2(b) and (c)), the vibration modes offolic acid has been decreased, but at 400C the peaks dueto the CO folate disappeared because of the decomposi-tion of folic acid but appearing a relatively broad peakaround 1200 cm1 should be due to the some C-N or

C-OH vibrations of adsorbed specious on NiO surfacesduring the calcination time, but by increasing tempera-ture up to 900C this peak is disappeared. Two newpeaks were also found at 490 and 445 cm1(Figure 2(d)),these peaks undoubtedly assigned to Ni-O stretching aswas reported earlier by other researches [36,37].

3.2. SEM and TEM Studies

The SEM images of as prepared nickel-folic acid hybridwith molar Ratio 1/1 after refluxing for 6 h, 12 h, fol-lowed by calcinations at 400C designated as NiO400and EDX of NiO400 are given in Figures 3(a)-(d) re-

spectively. As seen in Figure 3(a), the SEM image of asprepared sample does not show any obvious morphologybut by increasing reflux time from 6 h to 12 h the particle

Figure 2. FT-IR spectra of (a) Folic acid; (b) Heated at100C; (c) at 200C; and (d) at 400C.

Figure 3. Scanning electron microscopy of (a) As prepared

nickel-folic acid hybrid with molar ratio 1/1after refluxing

for 6 h; (b) Reflux for 12 h; (c) Reflux for 12 followed by

calcinations at 400C designated as NiO400; (d) EDX of

NiO400.

size appeared as 48 nm (Figure 3(b)). The best resultswas obtained after calcination at 400C with particle size21 - 22 nm. It was also observed increasing the amountof the folic acid from 1/1 to 5/1 the size of the nanoparti-

cles increases and increasing the reflux time, the particlesize decreases. The photographs show that the calcina-tion temperatures are important factor on particle sizeand distribution of the nanoparticles. The higher calcina-tion temperature, results the smaller the particles and themore good distribution.

Therefore the NiO400 has been used for further studies.The EDX of NiO400 is also shown in Figure 3(d). Theinteresting point is no peaks due to the impurity is ap-peared.

The transmission electron microscopy (TEM) photo-graphs of NiO400has been given in Figure 4(a). The size

of the nanoparticles obtained from the XRD diffractionpatterns are in close agreement with the TEM studieswhich show sizes of about 4 - 5 nm. The selected areadiffraction (SAED) pattern of the NiO400 is shown inFigure 4(b), which shows the good crystalinity of thenanoparticles.

3.3. TGA/DTA

In order to reveal the changes that occurred during heattreatment of the precursor powders, TGA, and DTAanalysis of as prepared sample was carried out from 30Cto 750C in atmosphere (Figures 5(a)-(b)). According to


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Figure 4. Transmission electron microscopy (TEM) of (a)

NiO400, (b) SAED of NiO400.

Figure 5. (a) TGA; and (b) DTA of as obtained Ni precur-

sor.

the TGA curve Figure 5(a), the major part of the weightloss seems to occur below 400C. The TGA curve shows

a weight loss of 8% in the temperature range of 60C -140C due to the evaporation of the absorbed water. Anexothermic peak at approximately 342C occurs in DTA(Figure 5(b)), which might be associated with the con-version of precursor to NiO and also the decompositionof the organic residues. The total process has the weightloss of about 48.63%.

3.4. Nitrogen Sorption Studies

The nitrogen adsorption-desorption isotherms and poresize distribution of NiO calcined at 400C are shown in

Figures 6(a)-(b) respectively. Curved inflations at P/P

,0.4 - 1 is related to the pressure of capillary condensationbased on BHJ calculation. The obtained results indicatethat the NiO400 with surface area 138.1 m

2/g, pore vol-ume 0.09 cm3/g, and pore diameter 2.83 nm is formed.

3.5. UV-Vis Studies

The UV-vis spectra of NiO bulk, NiO400and NiO100areshown in Figures 7(a)-(c) respectively. Observing amaximum absorption at the region 300 nm for the NiO400is interesting point. The photoluminescence spectra ofNiO400 shows a maximum UV emission at 381 nm by

(a)

(b)

Figure 6. Nitrogen adsorption-desorption isotherm of (a)

NiO400, (b) pore volume distribution of NiO400.

Figure 7. UV-vis absorption spectrum of (a) NiO bulk; (b)

NiO calcined at 400C; (c) Nano NiO100.


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excitation beam at 280 nm, the obtained results are con-sistent with those reported before [38,39].

3.6. Photocatalytic Activity

The photocatalytic activity of nanoporous NiO was pre-pared by nickel acetate, sodium hydroxide and folic acidas template followed by heating at 100C and calcinationat 400C designated as NiO400were evaluated by the de-gredation of Congo red (CR) solutions (Figure 8). TheUV-vis spectrum of CR shows two maximum absorptionat the regions 347 and 497 nm. By illuminating UV lightto the aqueous CR solution the two bands due to the azolinkage and naphthalene ring are decreased in the time135 min. UV light illumination of the aqueous Congo redsolution in presence of prepared nano structured NiOcause the absorption bands of the dye in the visible re-

gion to decrease with time and finally to disappear, indi-cating the destruction of its chromophoric structure in thevicinity of the azo-linkage. This is accompanied by aparallel decrease of the intensities of the bands in the ul-traviolet region located at 347 nm, attributed to the naph-thalene ring. It was observed by increasing time up to135 min with NiO400the degradation were completed.

The photodegredation percentage versus photodegre-dation time in the presence of the mentioned catalyst andthe illuminating CR without catalyst are shown in Figure9. Based on the obtained results without using the cata-lyst 20% of Congo red was photodegreded after 1 h, but

using the catalyst increases the degredation up to 90% atthe same time. The photocatalytic efficiency was ex-pressed in terms of percent of degradation from the fol-lowing equation:

0 0

0 0

Percent of degredation 100

100

C C C

A A A

(2)

where, C0represents the initial concentration of the CR,Cis the concentration after illuminating by UV-vis light,

Figure 8. Variation of the UV absorption spectra of Congo

red solution in the presence of NiO400.

A0 is the initial absorbance, and A is the variable ab-sorbance. Without any catalyst, only a slow decrease inthe concentration of Congo red was detected under UVirradiation. The addition of catalysts leads to obvious

degradation of organic dyes. The reusability of NiO400was checked by consecutive repeated adsorption of thedye and testing the photoactivity of the sample for thenew degradation cycle (Figure 10). This procedure wasrepeated three times on the same sample as described forCongo red. It was found that photo degradation effi-ciency of CR slightly decreases with the recycling andremains almost constant after successive cycles, which ismore than 90% of that of the first recycling times.

4. Conclusion

The NiO nanoporous was synthesized using folic acid as

Figure 9. The curves of (a) Ln(C0/C) vs irradiation time

efficiency of photo degradation (X) as a function of time; (b)

at 497 nm.

Figure 10. Results of recycling experiment for NiO400.


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template. The synthesized nanoporous as nanoparticleswere found to be fully crystalline with uniform distribu-tion. Increasing the time of the reflux of the solution de-creased the size of nanoparticles and increasing the

amount of the folic acid increased the size of thenanoparticles. The experimental observation was sup-ported by SEM and TEM analysis. The experimentalresults demonstrated that the NiO400 had an excellentoptical property and higher photocatalytic activity thanthat of bulk NiO for degradation of Congo red under UVirradiation. In addition, this kind of NiO400may provideguidance for the application of NiO in the treatment oforganic pollutants. There are many advantages in thiswork as it uses as a green solvent, is a simple method,saves time, uses cheap available chemicals, and providessmaller nanoparticles of NiO.

5. Acknowledgements

The financial support from the University of Alzahra isgratefully acknowledged.

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Facile Synthesis and Characterization of Nanoporous NiO

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